Manufacture of camphene.



] .UNITEI) STATEFTENT OFFICE.

FRITZ KOCH, OF LONDON, ENGLAND.

MANUFACTURE OF CAMPHENE T 1111 whom it may concern:

Specification of Letters Patent. Application filed November 24. 1906. Serial No. 34%874.

racemes Nov. 12, 1907.

In the same way as described by this process, the

'Berit known that I, FRITZ KOCH, Ph. D., a citizen oi hydrochloric acid of the liquid remaining at the manu- Germany, residing in .London, in the county of Middlesex, England, have invented a new and useful Im- 5 provemeut-in the Process of Manufacture of Camphene, to be particularly described and ascertained in and by the following statement.

. 1n the Bulletin de la Socit Chimique dc Paris (3) 15, p. 37 1 and in the Berichte Vol. 29, p. 695, Reyschler describes a-process tor the manufacture of camphene by heating alkali phenolate, from which the water has .been' removed, with pinene hydrochlorid. Alsothe Badische Anilin-aud Soda-Fabrik otLudwigshafen am Rh. has described in their patent specification for England No. 16429 06) a process of manufacturing i camphene by heating pinene hydrochlorid with an l l 1 l facture of pinene hydrochlorid, which contains the latter in a large degree, may be disengaged, and the campheue formed thereby, utilized.;

Example 1': 1720 parts of pinenehydrochlorid, 1800 parts of phenol are heated with 600 parts of calciumoxid for G to 7 hours at 180 C in a vessel having an up- I right condenser, and camphe ne is afterwards distilled off until the residuum is nearly dry. Thedistiiled liquid requires to be agitated with an aqueous alkaline E solution to get rid of the phenol, which has been caraqueous solution of an alkali phenolate in auautoclave. 5

" I have discovered that by heating a mixture of phenol, calcium oxid and pinene hydrochlorid under ordinary or atmospheric pressure, camphene entirely free from chlorin can be obtained.

The calcium oxid, which I use, serves on the one haud to combine with the water contained in the phenol and generated during the reaction, on the other hand to disengage the hydrochloric acid.

It is liardlyncccssar'y to mention, that by using such a cheap agent as calcium oxid in place of the alkali used inthc'processcs already named above, it ispossible to cheapen very cdnsiderably the manufacture of camphene. Furthermore; the tedious operation of distilling off the water formed by the reaction, which is absolutely. necessary in Rcyschlers process, is altogether. dispe1 1se(l with in my present improvement.

Compared with the said process. of Badische Anilin and- Soda-Fabrik my present invention has the adyantage thatthe process is performed under ordinary orried away with it,whereupon the camphene becomes separated from the alkaline phenol solution.

Example 2: 1720 parts of pinene hydrochlorid, 1800 parts of phenol are heated with 1600 parts of bariumoxid, and the mixture treated in the manner described in the ioregoing Example 1'.

Example 3: 1720 parts of pinene hydrochlorid, 1800 parts of phenol are heated with 1100 parts'of strontiumoxid and the mixture treated in the manner described in the foregoing Example 1.

Example 4: 1720 parts of pinene hydrochlorid. 2700 parts of napthol are heated with 600 partsof calcium oxid and the mixture treated in the manner described in the foregoing Example 1. p

Example 5: 1720 parts of pinene hydrochlorid, 2700 parts of naphthol are heated with 1600 parts of bariumoxid and the mixture treated in the manner described in the foregoing Example 1.

Example 6: 1720 parts oi pinene hydrochlorid, 2700 parts oi uaphthol are heated with 1100 parts of strontiumoxid and the mixture treated in the .manner described in the foregoing Example 1.

Having thus fully described my invention, what-l claim as new and desire to secure by Letters Patent,

rsz-

A process for manufacturing cnniphenc free from chloriu consisting of heating together pinene hydrochlorld,

calcium oxid and phenol, distilling off the camphene so formed, and separating phenol therefrom by shaking out in aqueous alkaline solution.

In testimony whereof I have signed my name to this specification in the presence of two subscribing witnesses.

lmtcd this 30th day of October 1906.

FRITZ KOCH.

Witnesses H. D. Jameson, F. L. Rxim. 

